双核有机锡(Ⅳ)配合物[Ph_3Sn(CH_3OH)O_2CC_6H_4CO_2(CH_3OH)-SnPh_3]·2CH_3OH和[Ph_3SnS_2CN(CH_2CH_2)_2NCS_2SnPh_3]·2CH_3OH的合成、表征和晶体结构

利用三苯基氯化锡和对苯二甲酸二钠、哌嗪荒酸二钠在甲醇中反应 ,合成了双核有机锡 (Ⅳ )配合物 [Ph3 Sn (CH3 OH)O2 CC6H4 CO2 (CH3 OH)SnPh3 ]·2CH3 OH (1)和 [Ph3 SnS2 CN(CH2 CH2 ) 2 NCS2 SnPh3 ]·2CH3 OH (2 ) .通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征 .用X射线单晶衍射测定了这两个化合物的晶体结构 .化合物 1为单斜晶系 ,空间群P2 1/n ,a =1.5 199(5 )nm ,b =0 .90 0 0 (3)nm ,c =1.82 0 6 (6 )nm ,β =113.970 (5 )° ,Z =2 ,V =2 .2 75 5(13)nm3 ,Dc=1.413g/cm3 ,μ =1.146mm-1,F(0 0 0 ) =980 ,R1=0 .0 35 3,wR2 =0 .0 6 0 6 .化合物 2为单斜晶系 ,空间群P2 1/c,a =1.5 0 6 6 (5 )nm ,b =1.0 875 (4 )nm ,c =1.35 42 (5 )nm ,β =91.6 14(5 )°,Z =2 ,V =2 .2 178(14)nm3 ,Dc=1.498g/cm3 ,μ =1.35 1mm-1,F(0 0 0 ) =10 0 8,R1=0 .0 40 1,wR2 =0 .1148.在 1和 2的晶体中 ,锡原子呈五配位畸变三角双锥构型 .配合物 1由未配位的甲醇分子通过氢键作用形成二维网状结构     

四核铜配合物 [CuBrP(p-OCH_3Ph) _3]_4 ·1.5CH_3OH的合成和晶体结构

CuXP(p OCH3Ph) 3]4·1 .5CH3OH (X =Br,I)的合成和Cu4Br4C85.5H90 O1 3.5P4的晶体结构。该晶体属于三方晶系 ,空间群为R3,晶胞参数为 :a =2 3.959(2 ) ,c =2 6.376(4) ,γ =1 2 0 .0 0°,V =1 31 1 2 (3) 3,μ(MoKα) =2 .92 1mm- 1 ,Z =6,Dc=1 .543g .cm- 3,F(0 0 0 ) =61 62 ,R =0 .0 4 1 9,wR =0 .0 792 .可观察衍射点 471 3个 (I 2σ(I) )。该分子中 4个Cu原子和 4个Br原子构成立方烷结构 ,每个Cu与 3个Br原子 ,1个P(p OCH3Ph) 3中的P原子形成畸变四面体配位。     

双核有机锡配合物CH_2(SnPhBr_2)_2·2DMSO的合成及晶体结构

通过双 (苯基二溴化锡基 )甲烷CH2 (SnPhBr2 ) 2 与DMSO的配位反应或者双 (苯基二溴化锡基 )甲烷的双 (三唑 )甲烷配合物CH2 (SnPhBr2 ) 2 ·CH2 Tz2 与DMSO的配体取代反应 ,可以制得标题化合物。用X 射线衍射测定了该化合物的晶体结构。结果表明 ,该晶体属于单斜晶系 ,C2 /c空间群。分子式为C1 3H1 2 Br4Sn2 ·2 (C2 H6SO) ,Mr=881 .52 ,a =1 0 .0 4 0 (2 ) ,b =1 5.345(3) ,c =1 7.992 (4) ,β =1 0 5.99(3)°,V =2 665(1 ) 3,Z =4,Dc=2 .1 92Mg·m- 3,μ =7.9674mm- 1 ,1 31 4个可观测衍射点 (I≥ 3σ(I) ) ,最终结构偏离因子R =0 .0 4 2 ,Rw =0 .0 4 6。分子中 2个锡原子均为六配位的变形八面体构型 ,通过DMSO中的氧原子桥联 2个锡原子。     

一维链状高价锰配合物[Mn_2(C_7H_4O_3)_4(CH_3OH)_2]·4H_2O_2CH_3OH的合成与结构

合成了一维链状高价锰配合物[Mn2(C7H4O3)4(CH3OH)2]4H2O2CH3OH,并对其进行了IR、X-射线衍射、UV-Vis和TG-DSC等表征。单晶衍射结果表明,该配合物晶体属三斜晶型,空间群P?晶胞参数a=7.653(5),b=10.486(7),c=12.943(8),=103.24(1),?=104.55(1),?=110.11(1),V=885.4(9)3,Z=1。UV-Vis光谱在547nm有一个吸收峰,相应于Mn(Ⅳ)的d-d电子跃迁光谱。     

[NiCl(Ph_2PCH_2CH_2OH)_2Cl·H_2O]~+Cl~-和[Ni(Ph_2P(O)CH_2CH_2OH)_4]~(2+)[NiCl_4]~(2-)的合成及晶体结构

通过NiCl2·6H2O与双齿配体2-(二苯基膦)乙醇(Ph2PCH2CH2OH)或其氧化物2-(二苯基氧膦)乙醇[Ph2P(O)CH2CH2OH]的反应,制得两种结构新颖的阳离子型镍配合物[NiCl(Ph2PCH2CH2OH)2 (H2O)]+Cl-(1)和[Ni(Ph2P(O)CH2CH2OH)4]2+[NiCl4]2-(2).通过元素分析、31P核磁共振及X射线单晶衍射对配合物1和2的结构进行了表征.配合物1的晶体属单斜晶系,C2/c空间群,中心金属Ni具有六配位八面体几何构型.配合物2属四方晶系,I4(1)/a空间群,中心原子Ni与PO基团中的O配位形成平面四边形构型.     

光致发光配合物[Au_2(PPh_3)_2(μ-4,4′-bpy)](ClO_4)_2 and [Cu_2(PPh_3)_4(CH_3CN)_2(μ-4,4′-bpy)](BF_4)_2的合成和晶体结构

合成了两个在空气中稳定的Au(Ⅰ )和Cu(Ⅰ )配合物 ,并运用元素分析、红外光谱、荧光光谱和X射线单晶衍射结构表征 ,[Au2 (PPh3 ) 2 (μ 4 ,4′ bpy) ](ClO4 ) 2 (1) (4 ,4′ bpy为 4,4′ 联吡啶 ) ,单斜晶系 ,空间群P2 1c,晶胞参数a=1.2 2 5 5 (4 )nm ,b=0 .9973(3)nm ,c=1.85 0 6 (6 )nm ,β =10 1.732 (5 )°,V =2 .2 145 (11)nm3 ,Z =4,最终偏离因子R =0 .0 430 ,wR =0 .0 937.[Cu2 (PPh3 ) 4(CH3 CN) 2 (μ 4 ,4′ bpy) ](BF4 ) 2 (2 ) ,单斜晶系 ,空间群P2 1c,晶胞参数a =1.34 6 3(3)nm ,b =1.46 81(3)nm ,c =2 .0 6 0 8(4 )nm ,β =10 0 .387(4 )° ,V =4.0 0 6 6 (13)nm3 ,Z =2 ,最终偏离因子R =0 .0 45 0 ,wR =0 .116 3.两个双核配合物都是利用 4,4′ 联吡啶桥联配体 ,形成直线结构 ,直线的两端以PPh3 或CH3 CN为端基 .Au(Ⅰ )为 2配位 ,Cu(Ⅰ )为 4配位 .两个配合物均具有光致发光特性 ,其中配合物 1发光来自MLCT激发态 ,而配合物 2则是受配位金属影响的配体内部发光 .     

CRYSTAL STRUCTURE OF 3-NITRO-2, 6-BIS(4''''-BENZO-15-CROWN-5)-AMINOPYRIDINE POTASSIUM PICRATE HYDRATE METHANOL, (C_(33)H_(42)N_4o_(12)K)C_6H_2N_3o_7·H_2O ·CH_3OH

<正> The title compound, (C33H42N4O12K)C6H2N3O7·H2O·CH3OH,Mr = 1003. 98,space group P1,a=11. 458(2) ,b= 14. 565(6) ,c=15. 828(3) A ;α=63. 34 (2),β=74. 06(1),γ=81. 03(2)°,V=2268. 1 A3;Z = 2,Dx = l. 47g/cm3,λ=0. 71069 A (MoKa).The final R = 0. 041 for 1700 observed reflections (I≥3σ(I)). The molecule is sandwich-like, and the cation K+ is sandwiched between the two crown rings.     

簇合物〔WOS_3 Ag_3 Br(PPh_3)_3〕·(OPPh_3)的合成和晶体结构

报道了〔WOS3Ag3Br(PPh3) 3〕·(OPPh3)簇合物 (C72 H6 0 Ag3BrO2 S3P4W ,Mr=176 4.6 1)单晶的合成和结构。该晶体属于三方晶系 ,空间群为R3 ,晶胞参数 :a =16 .14 0 (3) ,c =2 3 .0 0 3(4) ,V =5 189.4(15 ) 3,μ(MoKα) =3 .2 98mm- 1 ,Z =3 ,F(0 0 0 ) =2 5 98,Dc=1.6 94g/cm3。独立衍射点 2 181,可观察衍射点 195 2 (I≥ 2σ(I) ) ,R =0 .0 496 ,wR =0 .12 48。该晶体由簇合物分子〔WOS3Ag3Br(PPh3) 3〕和以P为中心的扭曲四面体结构的中性分子OPPh3 构成 ,其中的簇合物分子的骨架为由1个W原子、3个S原子、3个Ag原子和 1个Br原子构成的立方烷状。W、O(1)和Br原子位于C3轴上。     

Hydrothermal Synthesis,Crystal Structure and Thermal Stability Properties of the Complex [Cd_2(phen)_2(C_(14)H_(11)O_3)_4(CH_3CH_2OH)]·(CH_3OH)·(H_2O)

A dinuclear cadmium complex [Cd2(phen)2(C14H11O3)4(CH3CH2OH)]·(CH3OH)·(H2O) has been synthesized with benzilic acid and 1,10-phenanthroline by hydrothermal method.The crystal structure was determined by X-ray diffraction with crystal parameters as follows:triclinic system with space group P1,a = 1.21298(10),b = 1.32586(11),c = 2.4815(2) nm,α = 76.2630(10),β = 81.4500(10),γ = 69.1700(10)o,V = 3.6143(5) nm3,Dc = 1.438 g/cm3,Z = 1,F(000) = 1600,the final GOOF = 0.937,R = 0.0521 and wR = 0.1328.In the title complex,the dinuclear structure is defined by carboxyl oxygen atoms adopting a monodentate bridged coordination mode.The coordination environment of Cd(Ⅱ) ion is CdO4N2,giving a distorted octahedral coordination geometry.TG analysis shows that the title complex is stable under 140 ℃.     

Synthesis and Crystal Structure of a Novel Bimetallic Porphyrin Complex Salt {[MnTPP(CH_3OH)_2]_3Fe(CN)_6}·13H_2O

A novel bimetallic porphyrin complex salt, {[MnTPP(CH3OH)2]3Fe(CN)6}13H2O (TPP = tetraphenylporphyrin), has been synthesized and structurally characterized by X-ray diffraction analysis. The crystal is of trigonal, space group R-3 with a = b = 31.0618(10), c = 11.8366(8) A, Z = 3, V = 9890.3(8) A3, C144H134FeMn3N18O19, Mr = 2641.36, Dc = 1.330 g/cm3, μ(MoΚα) = 0.463 mm-1, F(000) = 4131, R = 0.0525 and wR = 0.1382 for 3045 observed reflections (I > 2σ(I)). The title complex is composed of one [Fe(CN)6]3- anion, three [MnTPP(CH3OH)2]+ cations and thirteen water molecules, which are connected by multiform hydrogen bonds leading to a 3D supramolecular network structure.     

Solvothermal Syntheses and Crystal Structures of Two New Nonmetal Borates:C_4H_(10)N_2·B_6O_8(OH)_2 and (NH_3CH_2CH_2NH_3)B_5O_8(OH)

Two new borate compounds,C4H10N2·B6O8(OH)2 1 and (NH3CH2CH2NH3)B5O8-(OH) 2,have been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction,IR,elemental analysis and thermal analysis. Compound 1 crystallizes in the monoclinic system,space group P21/c,with a=8.3318(17),b=6.2118(12),c=12.479(3) ,β=108.96(3)o,V=610.8(2) 3,Mr=313.02,Z=2,Dc=1.702 g/cm3,μ=0.150 mm-1,F(000)=320,R =0.0387 and wR =0.0924. Its layered structure is linked by infinite covalently coordinated neutral sheets with 3,20-membered window system,which are built up from alternative B6O8(OH)2 subunits donated by two piperzazine nitrogen donors. 2 crystallizes in monoclinic,space group Cc,with a=6.7207(13),b=11.481(2),c=12.564(3) ,β=95.25(3)o,V=965.4(3) 3,Mr=261.18,Z=4,Dc=1.797 g/cm3,μ= 0.164 mm-1,F(000)=536,R=0.0396 and wR=0.0752. Its oxoborate structure is generated from the sheets of 3,9-membered boron rings bonded diamine molecules through electrostatic and H-bonding interactions to form a two-dimensional layered network.     

{Cu[H_2NC(CH_2OH)_3]_2}{Pic}_2·H_2O的合成与晶体结构

三羟甲基氨基甲烷与苦味酸(Pic)铜在乙醇水混合液中反应,制得少见的不对称氢键连接的超分子化合物{Cu[H2NC(CH2OH)3]2}{Pic}2?H2O。晶体属三斜晶系,空间群为P ,晶胞参数为a = 6.894(1),b = 8.219(1),c = 13.543(3) ? ?= 79.290(1),?= 8 3.36(2), ?= 84.590(1)埃轿狢20H30CuN8O22,V = 746.9(2) 3,Z = 1,Dc = 1.774 g/cm3,F(000) = 411,?= 0.844 mm-1,R = 0.0334,Rw = 0.0863。在配合物的结构单元中, Cu2+位于对称中心,分别与2个四齿配体(三羟甲基氨基甲烷)中的2个OH,1个NH2,三齿配位,呈笼状螯合。而另一个OH,因配体和中心离子构型的限制,不参与配位。     

Syntheses and Characterizations of （CH3CH2CH2CH2NH3）6（BiI6）（I）2I3 and （NH3CH2CH2NH3）2Bi2I10

The title compounds have been respectively synthesized by solution process and solvothermal reaction, and their crystal structures were determined by X-ray diffraction method. For （CH3CH2CH2CH2NH3）6（BiI6）（I）2I3 1, it crystallizes in tficlinic, space group P1^- with Mr = 2049.76, a = 8.5719（1）, b = 11.7461（3）, c = 15.700（1）A, V = 1451.4（1）A^3, Z = 1, Dc = 2.345 g/cm^3, F（000） = 924, μ（MoKα） = 8.907 mm^-1, T = 293（2） K, the final R = 0.0655 and wR = 0.0804 for 2399 observed reflections with I 〉 2σ（I）. For （NH3CH2CH2NH3）2Bi2I10 2, it crystallizes in monoclinic, space group P21/n with Mr= 1811.20, a = 8.434（4）, b = 13.862（6）, c = 13.362（6）A, V = 1499.9（12）A^3, Z = 2, Dc = 4.010 g/cm^3, F（000） = 1536,μ（MoKα） = 22.007 mm^-1, T = 293（2） K, the final R = 0.0584 and wR = 0.1451 for 1798 observed reflections with I 〉 2σ（I）. The structures of 1 and 2 contain halobismuthate monomer and dimers, respectively. It is noteworthy that the dimers and their organic counters in 2 connect each other by N…I hydrogen bonds to form a layered structure, and the electrostatic interactions and crystal packing forces between layers give rise to the packing of the crystal. The optical absorption spectra of 1 and 2 reveal the appearance of sharp optical gaps of 2.13 and 2.01 eV, respectively.     

Synthesis and Crystallographic Characterization of Complex [(CH_3)_3NCH_2CH_2N(CH_3)_3][HgI_4]·H_2O Containing Novel Cation

1 INTRODUCTION The crystal structures of several tetrahalogeno-mercurates (II) have been reported with a wide va-riety of stereochemical arrangements[1, . These stu- 2]dies have shown that the Hg atom…     

Preparation and Crystal Structure of a Charge-transfer Complex between an Organic Substrate and Molybdosilicic Acid [(CH_3)_2NH(CH_2)C_6H_5]_4SiMo_(12)O_(40)·2CH_3CN·H_2O

1 INTRODUCTION Photochromism of intermolecular complexes based on polyoxometalates has received increasing attention due to their potential applications in ma- terial science[1～3]. However, most studies of photo- chromism have been made in solution[4～7], and those in solid state are relatively less and only a few with photosenstivity properties have been studied crystal- lographically. The title compound has a light yellow color in the darkness and turns greenish when exposed to sunligh…     

Synthesis and Crystal Structure of {(PPh_3)_2CIRuCIRu(PPh_3) B_(10)H_8[OCH(CH_3)_2)]_2}

1INTRODUCTIONAlthoughseveralhundredpolyhedralmetallaboraneshavebeencharacterized,theincidenceofruthenaboranesisparticularlysurprising.(hThefirstpolyhedralruthenaboraneisstructurallytypifiedbythecompound[(PPh,)2RuB,,HS(OEt),j,whichisobtainedin40%yieldsfromthereactionbetweentRuCI,(PPh,),jandcloso-tB,,H,,j'--inCHCI,/EtOH.tZiWithCH,COOH/THFt'iandC,H,COOH/CH,CI,">insteadofCHCI,/EtOH,twocompoundsF{(PPh,)2Ru}~(p-MeCO,)3--(pH)z-{RuB,,H,}jand[(PPh,)2(PhCOO)RuB,,HSCljhav…     

CRYSTAL STRUCTURE OF [Eu(μ-CH_3COC-O)(CH3COO)_2(H_2O)_2]_2·4H_2O

<正> C12H34O20Eu2,Mr=802.30 triclinic, space group P1, a= 8.955(2), b=9.328(1), c=10.536(2) A,α= 91.74(2),β=113.87(2),γ=118.23(2), V=681.7(2)A,Dm(flotation in CC14/ BrCH2CH2Br)=1.95,DX(Z=1) =1.954g cm-3,λ(MoKα)=0.71069 A,μ=6.41 cm-1,F(OOO)=391.92, T =. 295°K,final RF= 0.032 for 7483 observed reflections with |F0|>3a(|Fo|). The compound is isostructural with the known erbium complex,the basic unit being a centrosymmetric dimer composed of two nine-coordinate polyhedra sharing a common edge. An O atom in one or the three bidentate acetato groups about each europium atom serves as a bridge between the metal centars. The dimeric units are linked by hydrogen bonds involving both ligand and lattice water molecules to form a three-dimensional network.     

CRYSTAL AND MOLECULAR STRUCTURE OF(μ-PhCH_2S)(μ-CH_3C(0)CH_2S)Fe_2(CO)_6

<正> The crystal and molecular structures of (μ-PhCH2S)(μ-CH3C(O)CH2S)-Fe2(CO)6 have been determined by X-ray diffraction technique. The complex has chemical formula of C16H12O7S2Fe2 and Mr=492.08. The crystals are tri-clinic, space group P1,with a=8.461(5), b=10.937(5), c=ll.419(4)A,α=81.61 (3), β=78.21(4),γ=71.04(4)°,V=974.5A3, Dc=1.68 gcm-3,μ(MoKα)=17.3cm-1, Z=2,F(000)=495.93. The final R was 0.038 for 2874 independent reflections.